THERMAL TREATMENT PROCESSES

Objectives
1) To investigate the conventional heat treatment procedures, such as quenching and
tempering, used to alter the properties of steels.
2) To study the effects of heat treatment on the microstructure and mechanical properties of
steels; microstructure will be investigated and hardness will be measured for heat treated
specimens.

Section I:
Processes

Introduction

to

Thermal

Treatment

Heat treatment is a controlled process used to alter the microstructure of materials such as
metals and alloys to impart properties which benefit the working life of a component, for
example increased surface hardness, temperature resistance, ductility and strength.

1.1.
Treatment:

Heat

The heat treatment process for steel and steel alloys is composed of three
steps:
a) Heating to a temperature at which austenite is formed
(austenitizing)
b) Rapid
(quenching)

cooling

c) Reheating to
(tempering)

stabilize

structure

Austenite is a solid solution of carbon in iron in a face centered cubic (FCC) crystalline structure
which is stable at elevated temperature. The temperature at which austenite formation occurs
depends primarily on carbon content of the steel. This temperature can be determined from
the phase equilibrium diagram for the particular steel composition. The material must be held at
the austenitizing temperature for a period of time to ensure completeness of the phase
transformation and homogeneous structure. The amount of time required is dependent on the size
and shape of the work piece as well as its composition.

After the time required for austenite formation, the material is rapidly cooled by quenching. Most
often, quenching is accomplished by immersing the material in oil or water although air quenching is
also used. Under conditions of rapid cooling, austenite transforms into an unstable (non equilibrium)
phase known as martensite. This phase is a supersaturated solution of carbon in iron in a body
centered tetragonal structure. Martensite is very hard, relatively brittle phase which provides the
ability of strengthening steel to very high levels. Quenching usually results in a structure composed of
martensite plus ferrite (solid solution of carbon in iron in body centered cubic structure) and iron

carbide (cementite). The proportions present after quenching depend on carbon content and
cooling rate. Higher carbon content and rapid cooling tend to produce larger proportions of
martensite.
Martensite is hard and brittle. In order to reduce brittleness, increase ductility, and relieve internal
stresses from rapid cooling step, the material is subjected to a second heating operation known as
tempering. The temperature for the tempering step must be below the austenite transformation
temperature and is usually between 400F and 800F. The resultant properties of the steel after
tempering depend on the time allowed for tempering as well as the temperature.
The microstructure produced by any of the above heat treatments can be deduced using Continuous
Cooling Transformation (CCT) diagrams, which are directly related to the Time Temperature
Transformation (TTT) diagrams for the specific steel being treated. Such a TTT/CCT diagram for
eutectoid steel is shown in Figure 1. Fe-C phase diagram is given at Fig.2.

Fig.1. The dashed lines form TTT diagrams and the solid lines form the CCT diagrams. It can be seen
that CCT diagram can be obtained by moving the TTT curves a little to the downward right.

Figure 2: Iron-Carbon Phase Equilibrium diagram. (Source: Material Science and Metallurgy, 4 th
edition, Pollack, Prentice-Hall 1988)

1.2.Difference
diagrams

between

TTT

and

CCT

The essential difference between both the diagrams is the method of cooling. In TTT diagrams,
after cooling to a transformation temperature, you keep the temperature constant until the
transformation of austenite to the required transformation product (usually pearlite or bainite)
is complete and then cool to the room temperature.
In CCT diagrams, there is continuous cooling i.e. there is no holding of temperature. The
components are cooled at a constant or varying rates. The end products are usually
martensite or pearlite depending on the cooling media as well as the material of components.

Section II: Introduction to Characterization Tests

2.1. Hardness
Testing
Hardness tests measure the resistance to penetration of the surface of a material by a hard object.
The depth of penetration is measured by the testing machine and converted to a hardness number.

2.2. Microscopical
Examination
The microstructural study of a material can provide information regarding the morphology and
distribution of constituent phases as well as the nature and pattern of certain crystal imperfections.
Optical metallography is a basic tool of material scientists, since the equipment is relatively
inexpensive and the images can be obtained and interpreted easily. Distribution and morphology of
the phases can be studied and, if their properties are known, a quantitative analysis of the
micrographs provides some information about the bulk properties of the specimen. A limited study
of line and surface informations is also possible with the optical microscope. In order to obtain
reproducible results, with good contrast in the image, the specimen surface is polished and
subsequently etched with appropriate reagents before microscopic examination. In a polished
specimen, the etching not only delineates grain boundaries, but also allows the different phases to
be distinguished by differences in brightness, shape, and color of the grain.
Differences in contrast may result from differences in light absorption characteristics of the phases.
Etching results in preferential attack or preferential colouring of the surface. The preferential attack
is electrochemical corrosion; it is well known that different materials corrode at different rates. Grain
boundaries are often anodic to the bulk metal in the interior of the grain and so are etched away
preferentially and delineated. Staining is produced by the deposition of solid etch product on the
specimen surface. This is formed by chemical reaction between the etchant and the specimen. Under
favorable conditions the use of a proper etchant enables the identification of constituents. Failure
analysis depends a great deal on metallographic examination.
Microstructural examination can provide quantitative information about the following parameters:
1) The grain
specimens

size

of

2) The amount of interfacial area per unit

volume
3) The dimensions of constituent
phases

4) The amount and distribution of

phases.

2.2.1.

Specimen preparation for Microscopical Examination

Grinding
A small piece of specimen is cut by a metal-cutting-saw. After cutting operation, burrs on the edges
of the specimen should be carefully removed by a fine file or coarse grinding paper. The silicon
carbide grinding papers are held flat in a unit containing water facility for lubrication purpose. Each
unit contains four grades of papers, starting with grade 400 (coarse) and finishing with grade 1200
(fine). Grinding of the work piece is done by starting with the coarse papers and then continuing with
the fine papers. In each stage, grinding is done by rubbing the specimen backwards and forwards on
the grinding paper in one direction only, until the surface is completely ground, that is, until only
grinding marks due to this particular paper can be seen to cover the whole surface.
The specimen is washed thoroughly to remove coarse silicon carbide particles before proceeding
to a finer paper. The direction of grinding is changed from paper to paper, so that the removalof
previous grinding marks is easily observed. The extra time spent on each paper should be
increased as the finer papers are used. At the end of the grinding sequence, the specimen is
washed thoroughly and dried. Now, the specimen is ready for polishing.
Polishing
The polishing is done on rotating wheels covered by a special cloth. Alumina is employed as polishing
agent. The 1-micron size is commonly used, but the total polishing time shortened by starting on the
7 or 3 micron grade. The pad should be kept well supplied with lubricant. The specimen should be
held firmly in contact with the polishing wheel, but excessive pressure should be avoided. During
polishing the specimen should be rotated or moved around the wheel so as to give an even polish.
The specimen should be thoroughly cleaned and dried between each wheel.
Etching
Before etching, it is essential to ensure that the polished surface is grease and smear free. If the
final polishing has involved the use of magnesia ( in the form of an aqueous paste of fine
magnesia) or alumina (in the form of an aqueous suspension of fine alumina), then thorough
washing followed by drying off with acetone or alcohol will give a suitable surface, although it
must not be fingered afterwards.
Etching is generally done by swabbing. Etching times will vary from specimen to specimen, however,
a good general, procedure is to observe the surface during etching, and to remove the specimen
when evidence of the grains first appears. Microscopical examination will then reveal whether the
degree of etching is sufficient. Further etching can then follow to strengthen up the details as
required. After each etching, the specimen should be thoroughly washed in running water, followed
by drying off with acetone or alcohol.
* As a guide the following etchants are commonly used:
Alcoholic Ferric Chloride -copper alloys

Mixed Acids -aluminum alloys

Nital (ethyl alcohol+ 2% HN03) -iron and steel
Dilute HCI -zinc alloys

2.3. Roughness
Measurements
Roughness is a measure of the texture of a surface. It is quantified by the vertical deviations of a real
surface from its ideal form. If these deviations are large, the surface is rough; if they are small the
surface is smooth. Roughness is typically considered to be the high frequency, short wavelength
component of a measured surface (see surface metrology).Roughness plays an important role in
determining how a real object will interact with its environment. Rough surfaces usually wear more
quickly and have higher friction coefficients than smooth surfaces. Roughness is often a good
predictor of the performance of a mechanical component, since irregularities in the surface may
form nucleation sites for cracks or corrosion. Although roughness is usually undesirable, it is difficult
and expensive to control in manufacturing. Decreasing the roughness of a surface will usually
increase exponentially its manufacturing costs. This often results in a trade-off between the
manufacturing cost of a component and its performance in application.
Measurement. Roughness may be measured using contact or non-contact methods. Contact
methods involve dragging a measurement stylus across the surface; these instruments
include profilometers. Non-contact methods include interferometry, confocal microscopy,
electrical capacitance and electron microscopy.

Principle of a contacting stylus instrument profilometer: A cantilever (1) is holding a small tip (2) that
is sliding along the horizontal direction (3) over the object's surface (5). Following the profile the
cantilever is moving vertically (4). The vertical position is recorded as the measured profile (6) shown
in light green.

Sketch depicting how a probe stylus travels over a surface.

For 2D measurements, the probe usually traces along a straight line on a flat surface or in a
circular arc around a cylindrical surface. The length of the path that it traces is called the
measurement length. The wavelength of the lowest frequency filter that will be used to analyze
the data is usually defined as the sampling length. Most standards recommend that the
measurement length should be at least seven times longer than the sampling length. The
assessment length or evaluation length is the length of data that will be used for analysis.
Commonly one sampling length is discarded from each end of the measurement length.
Roughness Parameters. Each of the roughness parameters is calculated using a formula for
describing the surface. There are many different roughness parameters in use, but Ra is by far the
most common. Other common parameters include Rz, Rq, and Rsk. Some parameters are used only
in certain industries or within certain countries. For example, the Rk family of parameters is used
mainly for cylinder bore linings, and the motif parameters are used primarily within France.
Since these parameters reduce all of the information in a profile to a single number, great care
must be taken in applying and interpreting them. Small changes in how the raw profile data is
filtered, how the mean line is calculated, and the physics of the measurement can greatly affect
the calculated parameter.
Amplitude Parameters. Amplitude parameters characterize the surface based on the vertical
deviations of the roughness profile from the mean line. Many of them are closely related to the
parameters found in statistics for characterizing population samples. For example, Ra is the
arithmetic average of the absolute values and Rt is the range of the collected roughness data points.

Section III: Heat Treatment Exercise

1. Supply three SAE 1040 or 1080 or 4140 specimens (and the Jominy Bar).
Austenitize these at proper temperature (look at Fe-C phase diagram) for 1 hour.
Allow adequate time for the crucible to heat to the temperature of the furnace (about
10 minutes). A total of 1 hour heating time should be adequate allowing roughly 4550 minutes of soaking.
2. Normalizing - Rapidly remove one specimen and allow it to cool in air on a
ceramic base.
3. Quench Hardening Rapidly remove four specimens and quench them in
water at room temperature.
4. Tempering Reheat three of the water quenched specimens to 500 0C in another
furnace for 30 minutes, then remove it and allow it to cool in air to room temperature.

Section
Results

IV:

Tests

and

1. Determine the Rockwell hardness values for each of the heat treated
specimens after cleaning one of the surfaces with sand paper to remove any
hard carbon deposits that may have formed on the surface. Take 5 readings on
each sample.
2. Record these readings in Table 1.

Table 1: Hardness Rockwell C for heat treated AISI 1080 Steel

Measurement
Number
1
2
3
4
5
Mean Value

Normalized

Quenched

Tempered at
500 0C

3. Examine each specimen and sketch typical microstructure by means of optical

microscopy.
Specimens are going to be polished and etched as explained above.
4. Put microstructure photos with correct magnification bar.
5. Measure the surface roughness after each grinding step.
6. Record these readings in Table 2.

Table 2. Roughness measurement of normalized steel

Measurement
Number
1
2
3
Mean Value

After 400
grit grinding

After 800
grit grinding

After
polishing

Section V: Discussion
1. Discuss the expected microstructures and properties for each of the
specimens based on the appropriate TTT and/or CCT diagrams for the
cooling sequences applied.
2. Discuss the relationship between heat treatment and the resulting
hardness and microstructure obtained in this experiment.
3. Compare and comment on the experimental results obtained with
respect to the expected microstructure and hardness results.
4. When Austempering steel, after the 30 minutes in the 400C bath the
specimen is
removed from the bath and can be either quenched in water or allowed to air cool at
room temperature. Will these two procedures produce different results? Explain.
5. What is decarburization? What causes it and how is it prevented? How does
it affect the properties of heat treated steels?
6. What is purpose the surface roughness measurement?
7. What are the different methods to measure the roughness of a surface?

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